Bone-like Carbonated Apatite Titanium Anodization Coatings Produced in Citrus sinensis-Based Electrolytes
Source abstract
Abstract
Enhancing osseointegration is a common goal for many titanium implant coatings, since the naturally forming oxides are often bioinert and exhibit less than ideal bone-to-implant contact. Oxide coating surface topographies, chemistries, and crystallinities are known to play key roles in enhancing bone–implant interactions. In the present study, two novel anodization processes were developed in electrolytes based on juiced navel oranges to create bioactive oxide coatings on commercially pure titanium (CPTi) surfaces. Both oxide groups revealed multi-scaled micro and nano surface topographies, significant Ca and P-dopant incorporation exhibiting Ca/P ratios similar to human bone (1.7 and 1.8), and physiologically relevant Mg uptake levels of <0.1% and 1.4 at%. XRD and FTIR analyses of each oxide revealed a combination of tricalcium phosphate and hydroxyapatite phases that showed carbonate substitutions indicative of bone-like apatite formation. Finally, VDI indentation testing revealed good adhesion strengths, minimal cracking, and no visible delamination for both oxides. In summary, the anodization processes in the present study were shown to produce carbonated tricalcium phosphate and apatite containing oxides with contrasting levels of Mg uptake that show much promise to improve future implant clinical outcomes.
Source: crossref · Quality: baseline
Research context
OpenAlex topics: Bone Tissue Engineering Materials · Dental Implant Techniques and Outcomes · Magnesium Alloys: Properties and Applications
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
Affiliations
Department of Biomedical Materials Science, University of Mississippi Medical Center, Jackson, MS 39216, USA
Funding
University of Mississippi Medical Center
References (45)
Show source-provided references
1. Advanced surface engineering of titanium materials for biomedical applications: From static modification to dynamic responsive regulation
2. Evolution of anodised titanium for implant applications10.1016/j.heliyon.2021.e07408 ↗
3. Influence of altered Ca-P based electrolytes on the anodised titanium bioactivity10.1016/j.surfcoat.2021.127041 ↗
4. An updated review on surface functionalisation of titanium and its alloys for implants applications10.1016/j.matpr.2021.01.499 ↗
5. In vitro surface efficacy of CaP-based anodised titanium for bone implants10.1016/j.surfin.2023.102872 ↗
6. Influence of surface structures on biocompatibility of TiO/HA coatings prepared by MAO10.1016/j.matchemphys.2018.05.037 ↗
7. Deposition of novel bioactive nanoflower-like sodium titanate on TiO coating via anodic oxidation for biomedical applications10.1016/j.matlet.2018.01.115 ↗
8. Effect of Mg content on the bioactivity and biocompatibility of Mg-substituted fluorapatite nanopowders fabricated via mechanical activation10.1016/j.msec.2016.05.043 ↗
9. Jeong, J., Kim, J.H., Shim, J.H., Hwang, N.S., and Heo, C.Y. (2019). Bioactive calcium phosphate materials and applications in bone regeneration. Biomater. Res., 23.10.1186/s40824-018-0149-3 ↗
10. Anodized titanium with calcium and phosphorus surface enhancements for dental and orthopedic implant applications10.1016/j.tsf.2022.139117 ↗
11. Osteoblast response to nanostructured and phosphorus-enhanced titanium anodization surfaces10.1177/0885328219852741 ↗
12. Ciosek, Ż., Kot, K., Kosik-Bogacka, D., Łanocha-Arendarczyk, N., and Rotter, I. (2021). The Effects of Calcium, Magnesium, Phosphorus, Fluoride, and Lead on Bone Tissue. Biomolecules, 11.10.3390/biom11040506 ↗
13. Characterization and biocompatibility study of hydroxyapatite coating on the surface of titanium alloy10.1016/j.surfcoat.2019.07.067 ↗
14. Effect of doping in hydroxyapatite as coating material on biomedical implants by plasma spraying method: A review10.1016/j.ceramint.2020.10.112 ↗
15. Microstructure and mechanical properties of plasma sprayed HA/YSZ/Ti-6Al-4V composite coatings10.1016/j.biomaterials.2003.10.089 ↗
16. Formation mechanism and adhesive strength of a hydroxyapatite/TiO composite coating on a titanium surface prepared by micro-arc oxidation10.1016/j.apsusc.2015.11.086 ↗
17. Tite, T., Popa, A.C., Balescu, L.M., Bogdan, I.M., Pasuk, I., Ferreira, J.M.F., and Stan, G.E. (2018). Cationic Substitutions in Hydroxyapatite: Current Status of the Derived Biofunctional Effects and Their In Vitro Interrogation Methods. Materials, 11.10.3390/ma11112081 ↗
18. Carbonate substitution in the mineral component of bone: Discriminating the structural changes, simultaneously imposed by carbonate in A and B sites of apatite10.1016/j.jssc.2017.07.025 ↗
19. Hu, J., Shao, J., Huang, G., Zhang, J., and Pan, S. (2023). In Vitro and In Vivo Applications of Magnesium-Enriched Biomaterials for Vascularized Osteogenesis in Bone Tissue Engineering: A Review of Literature. J. Funct. Biomater., 14.10.3390/jfb14060326 ↗
20. Biosynthesis of TiO2 nanostructures using Camellia sinensis extract (polyphenols) and investigation of their execution as photoanodes in photovoltaic device10.1016/j.surfin.2024.104154 ↗
21. Titanium Anodization in Psidium Guajava10.33448/rsd-v11i12.34953 ↗
22. Parekh, A., Moore, M., Janorkar, A.V., and Roach, M.D. (2024). Mg-Doped Carbonated Hydroxyapatite and Tricalcium Phosphate Anodized Coatings on Titanium Implant Alloys. Appl. Sci., 14.10.3390/app142411831 ↗
23. Parekh, A., Knotts, P., Janorkar, A.V., and Roach, M.D. (2025). Citrus Fruit-Based Calcium Titanate Anodization Coatings on Titanium Implants. Oxygen, 5.10.3390/oxygen5020007 ↗
24. Parekh, A., Tahincioglu, A., Walters, C., Chisolm, C., Williamson, S., Janorkar, A.V., and Roach, M.D. (2025). Citrus-Fruit-Based Hydroxyapatite Anodization Coatings on Titanium Implants. Materials, 18.10.3390/ma18051163 ↗
25. Comparative study on chemical components of Gannan navel orange in different maturity stages based on UPLC-QTOF-MS metabolomics10.1016/j.focha.2023.100472 ↗
26. Zhang, J., Liu, Z., Luo, Y., Li, X., Huang, G., Chen, H., Li, A., and Qin, S. (2022). The Role of Flavonoids in the Osteogenic Differentiation of Mesenchymal Stem Cells. Front. Pharmacol., 13.10.3389/fphar.2022.849513 ↗
27. Kaempferol-immobilized titanium dioxide promotes formation of new bone: Effects of loading methods on bone marrow stromal cell differentiation in vivo and in vitro10.2147/IJN.S150786 ↗
28. Gorman, D., Green, C., Booth-Downs, F., Gee, M., and Fry, T. (2022). Rockwell Indentation Test for Evaluation of Adhesion of Coatings-aka Daimler-Benz Adhesion Test, National Physical Laboratory.10.47120/npl.MAT107 ↗
29. Oss Giacomelli, R., Mattos, J., Soprano, P., Salvaro, D., Binder, C., Klein, A., and Biasoli de Mello, J.D. (2014, January 21–24). Assessment of Multifunctional Coating Adhesion: Comparison Between Indentation and Scratch Tests. Proceedings of the 2nd International Brazilian Conference on Tribology, Foz do Iguaçu, Brazil.10.5151/1472-5836-25743 ↗
30. Drobný, P., Mercier, D., Koula, V., Škrobáková, S.I., Čaplovič, Ľ., and Sahul, M. (2021). Evaluation of Adhesion Properties of Hard Coatings by Means of Indentation and Acoustic Emission. Coatings, 11.10.3390/coatings11080919 ↗
31. Safari, B., Aghanejad, A., Roshangar, L., and Davaran, S. (2021). Osteogenic effects of the bioactive small molecules and minerals in the scaffold-based bone tissue engineering. Colloids Surf. B Biointerfaces, 198.10.1016/j.colsurfb.2020.111462 ↗
32. Advances in implant surface modifications to improve osseointegration10.1039/D1MA00675D ↗
33. Engineered functional doped hydroxyapatite coating on titanium implants for osseointegration10.1016/j.jmrt.2023.09.239 ↗
34. Magnetic Silicium Hydroxyapatite Nanorods for Enhancing Osteoblast Response in Vitro and Biointegration in Vivo10.1021/acsbiomaterials.9b00073 ↗
35. Phase stability and biological property evaluation of plasma sprayed hydroxyapatite coatings for orthopedic and dental applications10.1016/j.actbio.2015.01.022 ↗
36. Mechanical properties of sol-gel calcium titanate bioceramic coatings on titanium10.1016/j.surfcoat.2007.07.091 ↗
37. Cerqueira, A., García-Arnáez, I., Romero-Gavilán, F., Azkargorta, M., Elortza, F., Martín de Llanos, J.J., Carda, C., Gurruchaga, M., Goñi, I., and Suay, J. (2022). Complex effects of Mg-biomaterials on the osteoblast cell machinery: A proteomic study. Biomater. Adv., 137.10.1016/j.bioadv.2022.212826 ↗
38. Theophile, T. (2012). Research of Calcium Phosphates Using Fourier Transform Infrared Spectroscopy. Infrared Spectroscopy-Materials Science, Engineering and Technology, IntechOpen. Chapter 6.
39. One-step synthesis of petal-like apatite/titania composite coating on a titanium by micro-arc oxidation10.1016/j.matlet.2010.11.050 ↗
40. Surface characterization, shear strength, and bioactivity of anodized titanium prepared in mixed-acid electrolytes10.1016/j.surfcoat.2017.07.010 ↗
41. The significance of the surface properties of oxidized titanium to the bone response: Special emphasis on potential biochemical bonding of oxidized titanium implant10.1016/S0142-9612(03)00261-8 ↗
42. Effect of titanium dioxide intermediate layer on scratch and corrosion resistance of sol-gel-derived HA coating applied on Ti-6Al-4V substrate10.1007/s40204-021-00169-0 ↗
43. Morphological, mechanical and antibacterial properties of Ti-Cu-N thin films deposited by sputtering DC10.1016/j.heliyon.2023.e17170 ↗
44. Effect of pulsed electron beam treatment on the physico-mechanical properties of hydroxyapatite-coated titanium10.1016/j.ceramint.2015.09.092 ↗
45. Hydroxyapatite coatings prepared by micro-arc oxidation in Ca- and P-containing electrolyte10.1016/j.surfcoat.2006.07.052 ↗